Spinning assistants



Patented Nov. 29, 1949 SPINNING ASISTANTS Sanford A. Moss, Jr., Riz iley Park, Pa., assignor to American Viscose "Srporation, Wilmington, Del., a corporation or Delaware No Drawing.

Original application May 28, 1942,

Serial No. 444,903. Divided and this application January 12, 1946, Serial No. 640,981

3 Claims.

This invention relates to the manufacture of films, filaments and the like by extruding solutions of material to be formed into a coagulating or precipitating medium. This application is a division of my copending application Ser. No. 444,903, filed May 28, 1942, now abandoned.

This invention concerns a novel process of forming artificial filaments, films and related shaped articles by extruding solutions of the materlal to be formed, such as viscose, into an aqueous coagulating or precipitating bath and it also concerns a novel coagulating or precipitating bath Ior carrying out the process.

it is an object of the invention to improve the conditions of extrusion and of coagulation or precipltation during the formation or filaments, films and the like to insure that products of uniformly high quality are obtained. Other objects of the invention will be apparent from the description hereinafter.

The process and spinning bath of this invention may be employed in the iormation oi filaments, 1111115 and the like from various solutions, such as those viscose, or related cellulosic derivatives, and OI proteinous material, such as casein, but it will be described hereihaiter with relation to the spinning oi viscose.

in accordance with this invention, a solution oi the material from which the filaments and the like are to be Iormed is extruded through an 011E063 or a plurality thereof or tne appropriate cross-sectional shape into a coagulating or precipitating bath containing dissolved therein a condensation product of ethylene oxide with a polyhydric alcohol selected from the group consisting or sugars and those having the iormula RCnzUl-l where R is selected irom the group consistihg of (-Clrl'0I-l) 111-1 and inner ether anhydrldes threoi' Where 1:. is an integral number from 2 to b, which product contains at least nine ethylene oxide units per molecule of alcohol. The compounds are derived from the folowmg representative polyhydric alcohols: glycerol, erythritols, pentahydric alcohols, hexahydric alcohols such as mannitol, sorbitol, dulcitol, heptahydric alcohols, as well as such related compounds as the sugars, for example glucose, sucrose, and the like, and anhydro derivatives of the polyhydric alcohols, such as mannitan, sorbitan, mannide, and sorbide. All of these condensation products are water soluble and non-ionogenic. Concentrations of the condensation product within the spinning bath may range from as low as 0.001% to 0.01% up to the limit of solubility of the product therein.

. Spinning in the presence of these ethylene oxide products as spinning assistants improves the quality of the products obtained, insuring uniformity and reducing to a minimum any tendency of the filaments to break during spinning. This tendency of the filaments to break during spinning is particularly accentuated at high spinning speeds, such as of the order of from 2500 to 8000 inches per minute, and is particularly pronounced when attempts are made to spin viscose containing a high proportion of combined carbon disulphide, particularly at the above-mentioned high speeds. By high carbon disulfide content is meant a viscose containing more than 35% combined CS2 based on the alpha cellulose, such as between about 36 to higher. The spinning of high tenacity yarns from viscose, such as from viscose containing a high content of combined carbon disulphide, at high speed is in general accompanied by considerable breakage difiiculties, which result in what is termed slugging. The ends of the broken filaments tend to gather upon the adjacent unbroken portions of yarn and give rise to trouble during spinning, especially during the collecting of the filamentary, material in centrifugal spinning buckets, where such partially broken yarn frequently becomes wrapped around the tip of the funnel guide which directs the filamentary material into the spirming bucket. Besides the spinning difficulties which accompany the filament breakage and slugging, the yarn obtained when such breakage occurs is of definitely inferior quality. These spinning difiiculties are not to be attributed to clogging since they occur even when the spinneret orifices are entirely free of clogging, though any clogging tends to aggravate them.

An additional advantageous efiect distinct from that just described is accomplished by spinning in the presence of these ethylene oxide products, namely, the tendency to form solid deposits of irregular shape within the orifices is minimized. For this purpose, however, only those containing a great number of ethylene oxide units are entirely satisfactory. For example, it has been found necessary that the product contain at least on the order of about ethylene oxide units in order to obtain completely satisfactory results of this character, though those containing fewer of these units do show some slight improvement. When this clogging of some of the orifices is complete, it reduces the total number of filaments in the bundle issuing from a given spinneret and tends to make the remaining filaments somewhat larger in diameter than would be the case where no clogging of any of the orifices of the spinneret occurs. Where a number of the holes or orifices in the spinneret are only partially clogged, the result is a mixture of filaments of various sizes issuing from the spin-v neret. In addition, the filamentary bundle issuing from a given spinneret which is subject to clogging varies in uniformity along its length is a filamentary yarn having considerable nonuniformity within a given cross-section as well 2;

along its length. Other compounds have been Inents'at a speedof 2500 inches per minute into suggested for this purpose, such'as cation act'ive compounds and other ethylene oxide derivatives" of compounds containing a long chain hydro phobic group. As compared with these other compounds, those of this inventionhave the ad- 4 molecul was" substituted for the product in the bath of Example 1. The" concentration of the product in the bath was maintained at 0.007% during spinning.

Example 7 A viscose solution was extruded to form filaa spinning hath corresponding to that of Example unitsot ethylene oxide in the molecule was subvantage of being less rapidly exhausted from the bath under spinning conditions. Generally, at a given concentrationv of the assistant in the spinnin bath, roughly 7; as much of the compounds of this invention is consumed during spinning as would be consumed of the'compound's heretofore employed. Consumption as used here is meant to include the effects of instability, de-composition, and exhaustion.

The following examples are illustrative of' the invention Example 1 A viscose solution was extruded" into a spinning' bath comprising from 8 to 12% sulphuric aci'ctabout 20% sodium sulphate, about 5%-- zinc sulphate, and 0.01% or a condensation product of ethylene oxide with mannitol' containing 100 units of ethylene" oxide inthe molecule.

Example 2 I A Viscose solution was extruded into a spin-- ning. bath. containing from 7 to 9 sulphuric acid, about 14% sodium su1phate, about 1.% zinc sulphate,..;'eout 5% glucose, and 0.01 of a con-; densation product of ethylene oxide with mannitol containing. 100 units of ethylene oxide in the molecule.

Example 3 A viscose solution was extruded into a spin: ning ha having the composition of. Example 2 except that a concentration of'0.0'02% of 'a conoxide with glycerol having 9- units of ethylene oxide in the molecule.

Example 5 Av viscose solution was extruded at a: speed of about 2000 inches per minute into' aspinningbathhaving the composition of Example. 12 with the exception that an ethylene oxide condensation product with mannitol having. 18 ethylene oxide units was substituted for that in the bath of Example 1. The product was employed in 0.05% concentration.

Example 6 A viscose solution was extrudedinto" a spinnin bath corresponding to the composition of that in Example 1 with the exception that a condensation product of" ethylene oxide with glycerol-having 50' units of ethylene oxide in the stituted for the product in the bath of Example 1', theproduct being maintained in the bath at a concentration of 0.1

Example 8 Viscose solutions having various proportions of CS2" in the range from 35% 1 10-4570" were ex truded under the conditions of Example '7. ex cept thatthe spinning. speeds Werechanged to 2500 to 8000 inches perminute.

Example 9 A viscose solution was extruded into a spinning hath having the composition of Example 2 except that a condensation product of ethylene oxide with glucose containing units of ethylene oxide in the molecule was substituted for the product'o'f Example 2.

Example 10 it viscose solution was" extruded into a spin ning' bathhaving the composition of Example 2 exceptthat a condensation-product of ethylene oxide with sucrose containing 50 unitsofe'thylene oxideinthe molecule wassubstituted for the product of- Example 2-.

While preferred embodiments of theinvention have been disclosed; it is tobe understood that changes andyariations may lee-made withoutde parting. from the spirit and scope of the invention as defined by the appended claims.-

What I claim is:

1. In the method of producing. filaments films 1 and the like, the step of. extruding a solution of viscose through a jet into an aqueous precipitating medium containing a condensation prodnot ofethylene oxide with glycerol. containing at least 9 ethylene oxide. units per molecule.

2. In the method of producing filaments,v films and the like, the step of extruding a solution ofviscose through a jet into an aqueous precipi-- tating medium containing. a condensation product of ethylene oxide with glycerol containing at least 50 ethylene oxide units per molecule.

3. An aqueous acid medium for precipitatingviscose extruded in the form of filaments, films and'the' like, saidmed'ium containing a condensation product of glycerol with ethylene oxide containing at least ethylen'e oxide units per molecule.

' SANFORD AZ MOSS; JR.

REFERENCES CITED The following references are of record in the file of this patent:

STATES PATENTS Cowling Mar. 26'; I946 Certificate of Correction Patent N 0. 2,489,310 November 29, 19 49 SANFORD A. MOSS, JR.

It is hereby certified that errors appear in the printed specification of the above numbered patent requiring correction as follows:

Column 1, line 24, before the Word viscose iiisert of column 2, line 12, before hlgher insert or; and that the said Letters Patent should be read with these corrections thereiifthat the same may conform to the record of the case in the Patent Ofiice.

Signed and sealed this 23rd day of May, A. D. 1950.

THOMAS F. MURPHY,

Assistant Gammissz'oner of Patents. 

